Hydrochloric Acid → 7-Amino-1-(1-piperazinyl)-naphthalene

HRID 235151노트

반응식

HRID 235151 반응식
C([NH:9][C:10]1[CH:19]=[C:18]2[C:13]([CH:14]=[CH:15][CH:16]=[C:17]2[N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:12][CH:11]=1)(=O)C1C=CC=CC=1.Cl>C(O)C>[NH2:9][C:10]1[CH:19]=[C:18]2[C:13]([CH:14]=[CH:15][CH:16]=[C:17]2[N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 189675377-Benzamido-1-(1-piperazinyl)-naphthalene2회

생성물 1

HCID 189675327-Amino-1-(1-piperazinyl)-naphthalene수율 47%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The product of Example 11 (7-benzamido-1-(1-piperazinyl)-naphthalene, (0.063 g, 0.19 mmol) was combined with hydrochloric acid in ethanol (4 mL) and refluxed 16 hours. The reaction was concentrated at reduced pressure and the residue was neutralized with 4 N sodium hydroxide and extracted with methylene chloride. The organic phase was washed with brine, dried and concentrated to a tan solid (0.041 g). The solid was recrystallized from ethyl acetate/hexane to give 0.020 g (47%) of the title compound as light tan crystals. mp 184°-186° C. HRMS m/e calculated for C14H17N3 : 227.1419. Observed m/e 227.1405.

후처리

  1. temperaturerefluxed 16 hours
  2. concentrationThe reaction was concentrated at reduced pressure
  3. extractionextracted with methylene chloride
  4. washThe organic phase was washed with brine
  5. customdried
  6. concentrationconcentrated to a tan solid (0.041 g)
  7. customThe solid was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-ba7fe15075624f5d973b232c3674cecf
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05597826

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